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Preparation method of diallyl carbonate

A diallyl carbonate and carbonate technology, applied in the field of preparation of diallyl carbonate, can solve the problems of high toxicity of materials, serious environmental pollution, difficult control of materials, etc., and achieves low toxicity of materials and easy availability of raw materials , the effect of simple process

Inactive Publication Date: 2014-03-12
SHENZHEN CAPCHEM TECH CO LTD
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AI Technical Summary

Problems solved by technology

[0003] Among the synthetic methods of diallyl carbonate currently reported, one of the methods is that the reactant CO 2 Allyl alcohol and allyl alcohol need to be reacted under a certain pressure and a solvent, which requires high production equipment, and the control of materials in the reaction process also brings major problems to production; there are also reports in the literature that the reactants allyl alcohol and trichlorochloroformate Methyl ester reacts in ether solution under the catalysis of pyridine to generate diallyl carbonate. For the trichloromethyl chloroformate mentioned in this method, its alias is diphosgene, a colorless liquid, and it is easy to decompose and release phosgene when it meets heat or alkali. , Ether is also a volatile and explosive substance. In mass production, it is difficult to control the material, the material is highly toxic, and the environment is seriously polluted.

Method used

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  • Preparation method of diallyl carbonate

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Experimental program
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Effect test

Embodiment 1

[0026] In a 2000ml four-neck flask, add 581g (10.0mol) of propenyl alcohol and 11g (about 0.08mol) of potassium carbonate and stir evenly, then weigh 450g (5.0mol) of dimethyl carbonate and slowly drop it from a constant pressure dropping funnel. The temperature of the oil bath was controlled at about 85°C, and the reaction was carried out by magnetic stirring for 4 hours. During this process, the composition and content of light components evaporated from the reaction are as follows:

[0027] Methanol content: 27.89% (GC); Propylene alcohol content: 53.62% (GC); Dimethyl carbonate content: 9.67% (GC); Allyl methyl carbonate content: 7.87% (GC); Diallyl carbonate Ester content: 0.84% ​​(GC).

[0028] After the reaction solution was filtered to remove potassium carbonate, it was rectified under reduced pressure to obtain 352 g of diallyl carbonate, the content was 99.71% (GC), and the yield was 49.6%.

Embodiment 2

[0030] In a 2000ml four-neck flask, add 598g (10.3mol) of allyl alcohol and 12g of potassium carbonate (about 0.087mol) and stir evenly, then weigh 595g (5.04mol) of diethyl carbonate and slowly drop it from a constant pressure dropping funnel. Slowly raise the temperature of the oil bath to 95°C, and magnetically stir the reaction for 4h. Simultaneously, the mixture generated by the reaction in this process is steamed at normal pressure, and its composition and content are as follows respectively:

[0031] Ethanol content: 29.81% (GC); Propylene alcohol content: 47.63% (GC); Diethyl carbonate content: 12.66% (GC); Allyl methyl carbonate content: 7.99% (GC); Diallyl carbonate content Ester content: 1.89% (GC).

[0032] After the reaction solution was filtered to remove potassium carbonate, 316 g of diallyl carbonate was obtained after rectification under reduced pressure, with a content of 99.41% (GC), and a yield of 44.1%.

Embodiment 3

[0034] In a 2000ml four-neck flask, add 901g (15.5mol) of propenyl alcohol and 15g (about 0.11mol) of potassium carbonate and stir evenly, then weigh 681g (7.5mol) of dimethyl carbonate twice and slowly Slowly drop and stir with magnetic force, raise the temperature of the oil bath to 90°C, and react until no distillate flows out. The composition and content of the distillate are as follows:

[0035] Methanol content: 30.29% (GC); Propylene alcohol content: 50.63% (GC); Dimethyl carbonate content: 10.62% (GC); Allyl methyl carbonate content: 6.65% (GC); Diallyl carbonate Ester content: 0.96% (GC).

[0036] After the reaction solution was filtered to remove potassium carbonate, 563 g of diallyl carbonate was obtained after rectification under reduced pressure, with a content of 99.62% (GC), and a yield of 52.6%.

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Abstract

The invention aims to provide a preparation method of diallyl carbonate. The preparation method is safe, is low in cost, simple in separating and refining procedures and high in yield, and is used for preparing plenty of diallyl carbonate easily. The preparation method comprises the following steps of adding allyl alcohol and alkali metal catalysts to a reaction vessel in an inert dry atmosphere, dropwise adding carbonic ester after stirring the materials uniformly, controlling the temperature to be about 90 DEG C after dropwise adding, removing most generated light components through evaporation to obtain reaction mixed liquor, filtering the reaction mixed liquor to remove insoluble salt to obtain filtrate, then rectifying the filtrate at reduced pressure and collecting the fraction, thus obtaining diallyl carbonate with high purity.

Description

technical field [0001] The invention relates to a method for synthesizing and purifying an organic compound, in particular to a method for preparing diallyl carbonate. Background technique [0002] Diallyl carbonate is a new type of non-aqueous lithium-ion battery electrolyte additive, and it can also be used as a new type of linear carbonate solvent mixed with cyclic carbonate to obtain better performance. At the same time, diallyl carbonate is also an important polymer monomer. Due to its excellent transparency, it is often used in key parts of electrical or electronic equipment. Some allyl ester monomers are also widely used as crosslinkers for preformed polyester or mat adhesives in neat, pellet and premixed molding compounds, as well as in the processing of glass cloth and decorative laminates Forming. [0003] Among the synthetic methods of diallyl carbonate currently reported, one of the methods is that the reactant CO 2 Allyl alcohol and allyl alcohol need to be r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/96C07C68/06
CPCC07C68/06C07C69/96
Inventor 王帮应陈群汪仕华雷伟健王洪瑞
Owner SHENZHEN CAPCHEM TECH CO LTD
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